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Countercurrent Chromatographic Separation of Lipophilic Ascorbic Acid Derivatives and Extract fromKadsura coccineaUsing Hydrophobic Organic-Aqueous Two-Phase Solvent Systems
Journal of Liquid Chromatography & Related Technologies ( IF 1.3 ) Pub Date : 2009-09-04 , DOI: 10.1080/10826070903187981
Kazufusa Shinomiya 1 , Heran Li , Susumu Kitanaka , Yoichiro Ito
Affiliation  

Abstract Countercurrent chromatographic (CCC) separation of lipophilic ascorbic acid derivatives and the crude extract from Kadsura coccinea was performed using the type-J multilayer coil planet centrifuge with a hydrophobic organic-aqueous two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/aqueous 0.1% trifluoroacetic acid at the volume ratio of 5:5:6:2. The lipophilic ascorbic acid derivatives were separated in the order of L-ascorbyl 2,6-dibutyrate, L-ascorbyl 6-palmitate and L-ascorbyl 6-stearate by eluting the lower phase as the mobile phase, and L-ascorbyl 2,6-dipalmitate was separated by eluting the upper phase at the opposite direction. The above solvent system was then applied to the CCC separation of the extract prepared from K. coccinea. With lower phase mobile, the extract was mainly separated into two peaks corresponding to lignans and triterpenoids accordingly. The HPLC analysis of the fractions showed that the former peak contained Kadsulignan N, Schizandrin H and Neokadsuranin as lignans, and the latter peak, Micranoic acid A, Neokadsuranic acid B and beta-Sitosterol as triterpenoids. The overall results indicate that the hydrophobic organic-aqueous two-phase solvent system used in the present studies was useful for the CCC separation of lignans and triterpenoids present in the natural products.

中文翻译:

使用疏水性有机-水两相溶剂系统逆流色谱分离亲脂性抗坏血酸衍生物和 Kadsura coccinea 提取物

摘要 使用 J 型多层螺旋行星离心机和疏水性有机-水两相溶剂体系(由正己烷/乙酸乙酯/乙醇/0.1% 三氟乙酸水溶液,体积比为 5:5:6:2。亲脂性抗坏血酸衍生物按照 L-抗坏血酸 2,6-二丁酸酯、L-抗坏血酸 6-棕榈酸酯和 L-抗坏血酸 6-硬脂酸酯的顺序分离,以下层相为流动相,L-抗坏血酸 2,6 -二棕榈酸酯通过以相反方向洗脱上层相而被分离。然后将上述溶剂体系应用于从 K. coccinea 制备的提取物的 CCC 分离。具有较低的相流动性,提取物主要分离为木脂素和三萜相应的两个峰。馏分的HPLC分析表明,前一个峰含有木酚素N、五味子H和Neokadsuranin作为木脂素,后一个峰含有微克酸A、Neokadsuranic酸B和β-谷甾醇作为三萜类化合物。总体结果表明,本研究中使用的疏水性有机-水两相溶剂系统可用于天然产物中存在的木脂素和三萜类化合物的 CCC 分离。
更新日期:2009-09-04
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